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Sodium Iodide → Noradenalone hydrochloride

HRID 1091105
ノート
印刷プレビュー

反応式

HRID 1091105 の反応式
[Cl:1][CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([OH:12])[CH:6]=1)=[O:4].[I-].[Na+].[N-:15]=[N+]=[N-].[Na+]>CC(C)=O>[ClH:1].[NH2:15][CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([OH:12])[CH:6]=1)=[O:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 33557Sodium AzideHCID 668342-Chloro-3',4'-dihydroxyacetophenone

生成物 1

HCID 199831Noradenalone hydrochloride収率 50.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
40 °C

実験手順

10 g (53.6 mmol) of 2-chloro-3',4'-dihydroxyacetophenone was dissolved in 50 ml of acetone, and 600 mg (4.0 mmol) of sodium iodide and 5.23 g (80.5 mmol) of sodium azide were added thereto. The mixture was refluxed for 24 hours. The insolubles in the reaction solution were removed by filtration, and the filtrate was concentrated under reduced pressure. To the reaction solution, ethyl acetate was added, and the mixture was washed sequentially with water and with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the oily residue was dissolved in 100 ml of methanol and 13.6 ml of concentrated hydrochloric acid. 1.5 g of 10% palladium carbon catalyst was added to the solution, and the mixture was stirred under heating at 40° C. under a hydrogen gas stream for 5 hours. The reaction solution was filtered, and the filtrate was concentrated under reduced pressure. To the concentrated residue, actone was added, and the precipitated crystals were collected by filtration to obtain 5.5 g (yield: 50.4%) of 2-amino-3',4'-dihydroxyacetophenone hydrochloride.

後処理

  1. temperatureThe mixture was refluxed for 24 hours
  2. customThe insolubles in the reaction solution were removed by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. additionTo the reaction solution, ethyl acetate was added
  5. washthe mixture was washed sequentially with water and with a saturated sodium chloride aqueous solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure
  8. dissolutionthe oily residue was dissolved in 100 ml of methanol
  9. addition1.5 g of 10% palladium carbon catalyst was added to the solution
  10. filtrationThe reaction solution was filtered
  11. concentrationthe filtrate was concentrated under reduced pressure
  12. additionTo the concentrated residue, actone was added
  13. filtrationthe precipitated crystals were collected by filtration

出典と根拠

ORDレコード
ord-5de5646c18d64af099c28f4a5094a92f
出典データセット
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05084453

反応ノート

読み込み中…

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